JP6738160B2 - Soft magnetic flat powder and method for producing the same - Google Patents
Soft magnetic flat powder and method for producing the same Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims description 112
- 238000004519 manufacturing process Methods 0.000 title description 12
- 239000002245 particle Substances 0.000 claims description 33
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 229910002796 Si–Al Inorganic materials 0.000 claims description 4
- 239000006249 magnetic particle Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- 230000035699 permeability Effects 0.000 description 62
- 238000000034 method Methods 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 22
- 238000010438 heat treatment Methods 0.000 description 22
- 238000011049 filling Methods 0.000 description 9
- 229910001004 magnetic alloy Inorganic materials 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000009689 gas atomisation Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 238000005275 alloying Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 239000006247 magnetic powder Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- 238000009692 water atomization Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000004709 Chlorinated polyethylene Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910017060 Fe Cr Inorganic materials 0.000 description 1
- 229910002544 Fe-Cr Inorganic materials 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 240000005499 Sasa Species 0.000 description 1
- 229910008458 Si—Cr Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
- B22F2009/0828—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
- H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
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Description
本発明は、RFID等の10MHz帯前後で使用されるアンテナに用いられる軟磁性扁
平粉末およびその製造方法に関する。
TECHNICAL FIELD The present invention relates to a soft magnetic flat powder used for an antenna used in the vicinity of 10 MHz band such as RFID and a manufacturing method thereof.
従来、軟磁性扁平粉末を含有する磁性シートは、電磁波吸収体、RFID(Radio
Frequency Identification)用アンテナとして用いられてきた。また、近年では、デジタイザと呼ばれる位置検出装置にも用いられるようになってきている。このデジタイザには、例えば特開2011−22661号公報(特許文献1)のような電磁誘導型のものがあり、ペン形状の位置指示器の先に内蔵されるコイルより発信された高周波信号を、パネル状の位置検出器に内蔵されたループコイルにより読み取ることで指示位置を検出する。ここで、検出感度を高める目的で、ループコイルの背面には高周波信号の磁路となるシートが配置される。この磁路となるシートとしては、軟磁性扁平粉末を樹脂やゴム中に配向させた磁性シートや、軟磁性アモルファス合金箔を貼り合わせたものなどが適用される。磁性シートを用いる場合は、検出パネル全体を1枚のシートに出来るため、アモルファス箔のような貼り合せ部での検出不良などがなく優れた均一性が得られる。
Conventionally, a magnetic sheet containing a soft magnetic flat powder has been used for an electromagnetic wave absorber, an RFID (Radio).
It has been used as an antenna for frequency identification. Further, in recent years, it has come to be used also in a position detection device called a digitizer. This digitizer includes, for example, an electromagnetic induction type as disclosed in Japanese Unexamined Patent Application Publication No. 2011-22661 (Patent Document 1), in which a high-frequency signal transmitted from a coil built in the tip of a pen-shaped position indicator, The pointing position is detected by reading with the loop coil built in the panel-shaped position detector. Here, for the purpose of increasing the detection sensitivity, a sheet that serves as a magnetic path for high-frequency signals is arranged on the back surface of the loop coil. As the magnetic path sheet, a magnetic sheet obtained by orienting soft magnetic flat powder in resin or rubber, a sheet obtained by laminating a soft magnetic amorphous alloy foil, or the like is applied. When a magnetic sheet is used, the entire detection panel can be made into a single sheet, so that excellent uniformity can be obtained without detection failure at a bonded portion such as an amorphous foil.
また、従来、磁性シートには、Fe−Si−Al合金、Fe−Si合金、Fe−Ni合
金、Fe−Al合金、Fe−Cr合金などからなる粉末を、アトリッションミル(アトライタ)などにより扁平化したものが添加されてきた。これは、高い透磁率の磁性シートを得るために、いわゆる「Ollendorffの式」からわかるように、透磁率の高い軟磁性粉末を用いること、反磁界を下げるため磁化方向に高いアスペクト比を持つ扁平粉末を用いること、磁性シート中に軟磁性粉末を高充填することが重要であるためである。軟磁性扁平粉末の長径を大きくし、アスペクト比の高い扁平状の粉末を作製する方法として、例えば、特許第4636113号公報(特許文献2)には、炭素数2〜4の1価アルコールを用いて扁平加工を実施する方法が開示されている。
Further, conventionally, powders made of Fe-Si-Al alloys, Fe-Si alloys, Fe-Ni alloys, Fe-Al alloys, Fe-Cr alloys, etc. have been applied to magnetic sheets by an attrition mill or the like. Flattened ones have been added. This is because in order to obtain a magnetic sheet having a high magnetic permeability, as can be seen from the so-called "Ollendorff's equation", soft magnetic powder having a high magnetic permeability is used, and a flat surface having a high aspect ratio in the magnetization direction is used to reduce the demagnetizing field. This is because it is important to use the powder and to highly fill the magnetic sheet with the soft magnetic powder. As a method of increasing the major axis of the soft magnetic flat powder to produce a flat powder having a high aspect ratio, for example, Japanese Patent No. 4636113 (Patent Document 2) uses a monohydric alcohol having 2 to 4 carbon atoms. There is disclosed a method of performing flattening by using the above method.
デジタイザ機能はスマートフォンやタブレット端末などへ適用されるが、このようなモ
バイル電子デバイスは小型化の要求が厳しく、磁路シートとして用いられる磁性シートにも薄肉化の要求が高く、50μm以下程度の薄さのものが用いられるようになってきた。さらに、タブレット端末には液晶画面が10インチにもなるものがあり、磁性シートにも大面積が要求されるようになってきた。このような薄肉の磁性シートを一般的に適用される圧延やプレスによる方法で作製した場合、従来の厚さの磁性シートでは問題にならなかった。粉末のシート成形性が問題となるようになってきた。
Although the digitizer function is applied to smartphones and tablet terminals, such mobile electronic devices are required to be small in size, and the magnetic sheet used as a magnetic path sheet is also required to be thin, and the thickness is about 50 μm or less. The thing of Sasa came to be used. Further, some tablet terminals have a liquid crystal screen with a size of 10 inches, and a large area has been required for a magnetic sheet. When such a thin magnetic sheet is produced by a generally applied rolling or pressing method, the conventional magnetic sheet has no problem. Sheet formability of powders has become a problem.
すなわち、使用する軟磁性扁平粉末の長径が過大であるとき、50μm以下の薄さの磁性シートを作る際に、方向性が揃わなかったり、シート内の磁性粉末に粗密ができたりして、シート成型がうまくいかない場合が多い。シート成型時のこのようなトラブルをなくす為に、シート作製時の粉末充填率を下げるといった方法や成型後にシートをプレスするといった方法などが行われる。しかし、前者の方法などでは結果的にシートの透磁率を下げ性能を低下させる。また、後者の方法などではシート中の粉末に過大な応力がかかるために、粉末に歪が導入される。歪の導入は粉末の保磁力Hcの増大をもたらし、粉末の透磁率が低下するため、結果的に性能を低下させる。 That is, when the soft magnetic flat powder to be used has an excessively long diameter, when the magnetic sheet having a thickness of 50 μm or less is not formed, the directionality is not uniform, or the magnetic powder in the sheet is coarse and dense, In many cases molding does not go well. In order to eliminate such a trouble at the time of forming the sheet, a method of lowering the powder filling rate at the time of producing the sheet, a method of pressing the sheet after the forming, or the like is performed. However, the former method or the like eventually lowers the magnetic permeability of the sheet and lowers the performance. Further, in the latter method or the like, excessive stress is applied to the powder in the sheet, so that strain is introduced into the powder. The introduction of strain brings about an increase in the coercive force Hc of the powder, which lowers the magnetic permeability of the powder and consequently reduces the performance.
例えば、特許文献2に示すような、平均粒径D50が大きい軟磁性扁平粉末は、シート成
型において困難である。
For example, a soft magnetic flat powder having a large average particle diameter D 50 as shown in Patent Document 2 is difficult in sheet molding.
そこで、本発明は、平均粒径が小さくシート成形性に優れ、かつ高い透磁率を有する軟
磁性扁平粉末及びその製造方法を提供することを目的とする。その発明の要旨とするところは、Fe−Si−Al合金からなる、軟磁性粉末を扁平化処理することにより得られた扁平粉末であって、平均粒子径D50とタップ密度TDの比(D50/TD)が35〜92であり、扁平粉末の長手方向に磁場を印加して測定した保磁力が239〜479A/m、扁平粉末の厚さ方向に磁場を印加して測定した保磁力が、扁平粉末の長手方向に磁場を印加して測定した保磁力の2〜4.5倍、XRDの測定磁性粒子に起因するピークの最強ピーク(2θ=44±2°)に関して半価幅が0.3〜0.6である軟磁性扁平粉末。
Therefore, an object of the present invention is to provide a soft magnetic flat powder having a small average particle size, excellent sheet formability, and high magnetic permeability, and a method for producing the same. The gist of the invention is a flat powder obtained by subjecting a soft magnetic powder made of a Fe—Si—Al alloy to a flattening treatment and having a ratio (D) of an average particle diameter D 50 and a tap density TD. 50 /TD) is 35 to 92, the coercive force measured by applying a magnetic field in the longitudinal direction of the flat powder is 239 to 479 A/m, and the coercive force measured by applying a magnetic field in the thickness direction of the flat powder is , 2 to 4.5 times the coercive force measured by applying a magnetic field in the longitudinal direction of the flat powder, and the full width at half maximum is 0 with respect to the strongest peak (2θ=44±2°) of the peaks caused by the magnetic particles measured by XRD. A soft magnetic flat powder of 0.3 to 0.6.
また、上記軟磁性扁平粉末は、水アトマイズ法またはガスアトマイズ法またはディスクアトマイズ法と、溶融による合金化後の粉砕法のいずれかによる原料粉末作製工程と、前記原料粉末を扁平化する扁平加工工程と、前記扁平加工された粉末を真空またはアルゴン、窒素雰囲気のいずれかで、200〜500℃で熱処理する工程により実現可能である。 Further, the soft magnetic flat powder is a water atomizing method or a gas atomizing method or a disk atomizing method, a raw material powder manufacturing step by any one of pulverizing methods after alloying by melting, and a flattening step for flattening the raw material powder. It can be realized by a step of heat-treating the flattened powder at 200 to 500° C. in a vacuum or an atmosphere of argon or nitrogen.
上記条件を満足する軟磁性扁平粉末を用いることによって、RFID等の10MHz帯
前後で、透磁率μの実数部μ′が大きく、虚数部μ″が小さいアンテナを作製することが出来る。実数部μ′が大きいと通信距離を長くする特性があり、虚数部μ″が小さいとエネルギーロスを小さくする特性がある。ここで、透磁率μは実数部μ′と虚数部μ″によって複素透磁率(μ=μ′―jμ″)で表すことができるが、μ′の最大値が大きいほどμ″の値も大きくなる傾向にある。
By using the soft magnetic flat powder satisfying the above conditions, it is possible to manufacture an antenna having a large real part μ′ and a small imaginary part μ″ of the magnetic permeability μ around 10 MHz band such as RFID. If ′ is large, it has a characteristic of increasing the communication distance, and if imaginary part μ″ is small, it has a characteristic of reducing energy loss. Here, the magnetic permeability μ can be expressed by a complex magnetic permeability (μ=μ′−jμ″) by a real part μ′ and an imaginary part μ″. The larger μ′ is, the larger μ″ is. Tends to become.
Si含有量は、5.5〜10.5質量%であることが好ましく、6.5〜9.5質量%
がより好ましい。Si含有量が5.5質量%よりも小さい場合、結晶磁気異方性定数が過度に大きくなるため、磁性シートの透磁率が小さくなる。また、Si含有量が10.5質量%より大きい場合、粉末粒子の硬さを過度に上昇させてしまうため、偏平加工における結晶粒微細化を過度に促進させてしまい、粉末の保磁力が増大し、結果、磁性シートの透磁率が小さくなる。
The Si content is preferably 5.5 to 10.5% by mass, and 6.5 to 9.5% by mass.
Is more preferable. When the Si content is less than 5.5% by mass, the crystal magnetic anisotropy constant becomes excessively large, so that the magnetic permeability of the magnetic sheet becomes small. Further, when the Si content is more than 10.5 mass %, the hardness of the powder particles is excessively increased, so that the grain refinement in flattening is excessively promoted and the coercive force of the powder is increased. As a result, the magnetic permeability of the magnetic sheet decreases.
Al含有量は、4.5〜8.0質量%であることが好ましく、5.5〜7.0質量%が
より好ましい。Al含有量が4.5質量%よりも小さい場合、結晶磁気異方性定数が過度に大きくなるため、磁性シートの透磁率が小さくなる。また、Al含有量が8.0質量%より大きい場合、偏平粉末の飽和磁束密度が過度に低くなつため、磁性シートの透磁率が小さくなる。
The Al content is preferably 4.5 to 8.0 mass%, more preferably 5.5 to 7.0 mass%. When the Al content is less than 4.5% by mass, the crystal magnetic anisotropy constant becomes excessively large, so that the magnetic permeability of the magnetic sheet becomes small. On the other hand, when the Al content is more than 8.0 mass %, the saturation magnetic flux density of the flat powder becomes excessively low, so that the magnetic permeability of the magnetic sheet becomes small.
平均粒径D50は、35〜55μmであることが好ましく、40〜50μmがより好まし
い。平均粒径D50が35μmよりも小さい場合、扁平粉末のアスペクト比が小さくなるため、磁性シート形成時の透磁率が小さくなる。また、平均粒径D50が55μmよりも大きい場合、磁性シートの成形性が悪化する可能性がある。
The average particle diameter D 50 is preferably 35 to 55 μm, more preferably 40 to 50 μm. When the average particle diameter D 50 is smaller than 35 μm, the aspect ratio of the flat powder becomes small, so that the magnetic permeability at the time of forming the magnetic sheet becomes small. If the average particle diameter D 50 is larger than 55 μm, the moldability of the magnetic sheet may deteriorate.
タップ密度は、0.6〜1.0であることが好ましく、0.7〜0.9がより好ましい
。タップ密度が0.6よりも小さい場合、扁平加工工程に時間を要するためコスト高になる。また、タップ密度が1.0よりも大きい場合、磁性シートへの扁平粉末の充填率が低くなり、磁性シートとしての透磁率μが小さくなる。上記の条件で軟磁性扁平粉末を製造することによって、シート成型性がよく、透磁率の高い粉末を作製することができる。
The tap density is preferably 0.6 to 1.0, and more preferably 0.7 to 0.9. If the tap density is less than 0.6, the flattening process requires time, resulting in high cost. Further, when the tap density is higher than 1.0, the filling rate of the flat powder into the magnetic sheet becomes low, and the magnetic permeability μ as the magnetic sheet becomes small. By producing the soft magnetic flat powder under the above conditions, it is possible to produce a powder having good sheet moldability and high magnetic permeability.
本発明の軟磁性扁平粉末は、平均粒径D50とタップ密度TDの比(D50/TD)が35
〜92であることが好ましく、D50/TDが35〜80であることがより好ましく、D50/TDが40〜60であることが最も好ましい。D50/TDが35よりも小さい場合、扁平粉末のアスペクト比が小さく、更に磁性シートへの充填率が低くなるため、磁性シートとしての透磁率μが小さくなる。また、D50/TDが92よりも大きい場合、扁平粉末のアスペクト比は大きく、磁性シートへの充填率は高くなるため、磁性シートの成形性が悪化する可能性がある。
The soft magnetic flat powder of the present invention has a ratio (D 50 /TD) of the average particle diameter D 50 and the tap density TD of 35.
Is preferably to 92, more preferably D 50 / TD is 35 to 80, and most preferably D 50 / TD is 40-60. When D 50 /TD is smaller than 35, the aspect ratio of the flat powder is small and the filling rate into the magnetic sheet is low, so that the magnetic permeability μ as the magnetic sheet is small. Further, when D 50 /TD is larger than 92, the aspect ratio of the flat powder is large and the filling rate into the magnetic sheet is high, which may deteriorate the formability of the magnetic sheet.
本発明は、上記軟磁性扁平粉末の製造方法であって、アトマイズ法で作製された軟磁性
合金粉末を、扁平化する扁平加工工程と、不活性ガス中で熱処理する熱処理工程とを備える軟磁性扁平粉末の製造方法を提供する。
The present invention is a method for producing the soft magnetic flat powder, wherein the soft magnetic alloy powder produced by the atomizing method is provided with a flattening step for flattening and a heat treatment step for heat treatment in an inert gas. A method for producing a flat powder is provided.
<原料球状粉末準備工程>
本発明の軟磁性扁平粉末は、軟磁性合金粉末を扁平化処理することで作製することができる。また、軟磁性合金粉末は、飽和磁化の値が高い粉末であることがより好ましい。一般的に、保磁力と飽和磁化の値が優れているのは、Fe−Si−Al系合金である。
<Raw material spherical powder preparation process>
The soft magnetic flat powder of the present invention can be produced by flattening the soft magnetic alloy powder. Further, the soft magnetic alloy powder is more preferably a powder having a high saturation magnetization value. In general, Fe-Si-Al alloys have excellent coercive force and saturation magnetization values.
軟磁性合金粉末は、ガスアトマイズ法、水アトマイズ法、ディスクアトマイズ法といった各種アトマイズ法と溶融による合金化後の粉砕法のいずれかによって作製される。軟磁性合金粉末の含有酸素量は、少ないほうがより好ましいため、ガスアトマイズ法による製造が好ましく、さらに不活性ガスを用いての製造がより好ましい。ディスクアトマイズ法による方法でも問題なく製造出来るが、量産性の観点からは、ガスアトマイズ法が優れている。 The soft magnetic alloy powder is produced by any of various atomizing methods such as a gas atomizing method, a water atomizing method, a disk atomizing method and a pulverizing method after alloying by melting. Since the smaller the oxygen content of the soft magnetic alloy powder, the more preferable it is, the production by the gas atomization method is preferable, and the production using an inert gas is more preferable. Although the disk atomization method can be used for production without problems, the gas atomization method is superior from the viewpoint of mass productivity.
本発明に用いられる軟磁性合金粉末の粒度は特に限定されないが、扁平後の平均粒径を
調整する目的もしくは、含有酸素量の多い粉を除去する目的、その他、製造上の目的に応じて、分級されても良い。
The particle size of the soft magnetic alloy powder used in the present invention is not particularly limited, the purpose of adjusting the average particle size after flattening, or the purpose of removing powder with a large oxygen content, other, depending on the purpose of production, You may be classified.
<扁平加工処理工程>
次に、上記軟磁性合金粉末を扁平化する。扁平加工方法は、特に制限は無く、例えば、アトライタ、ボールミル、振動ミル等を用いて行うことができる。中でも、比較的扁平加工能力に優れるアトライタを用いることが好ましい。また、乾式で加工を行う場合は、不活性ガスを用いることが好ましい。湿式で加工する場合は、有機溶媒を用いることが好ましい。有機溶媒の種類については特に限定されない。
<Flat processing process>
Next, the soft magnetic alloy powder is flattened. The flattening method is not particularly limited, and can be performed using, for example, an attritor, a ball mill, a vibration mill or the like. Above all, it is preferable to use an attritor having relatively excellent flattening capability. Further, when dry processing is performed, it is preferable to use an inert gas. In the case of wet processing, it is preferable to use an organic solvent. The type of organic solvent is not particularly limited.
有機溶媒の添加量は、軟磁性合金粉末100質量部に対して、100質量部以上であることが好ましく、200質量部以上であることがより好ましい。有機溶媒の上限は特に限定されず、求める扁平粉の大きさ・形状と生産性のバランスに応じて適宜調整が可能である。また、酸素を低くするために、有機溶媒中の水分濃度は、有機溶媒100質量部に対して、0.002質量部以下での加工が好ましい。有機溶媒とともに扁平化助剤を用いてもよいが、酸化を抑えるために、軟磁性合金粉末100質量部に対して、5質量部以下であることが好ましい。
<熱処理工程>
The addition amount of the organic solvent is preferably 100 parts by mass or more, and more preferably 200 parts by mass or more with respect to 100 parts by mass of the soft magnetic alloy powder. The upper limit of the organic solvent is not particularly limited, and can be appropriately adjusted depending on the desired balance between the size and shape of the flat powder and the productivity. Further, in order to reduce oxygen, it is preferable that the water concentration in the organic solvent is 0.002 parts by mass or less with respect to 100 parts by mass of the organic solvent. Although the flattening aid may be used together with the organic solvent, it is preferably 5 parts by mass or less with respect to 100 parts by mass of the soft magnetic alloy powder in order to suppress oxidation.
<Heat treatment process>
次に、上記軟磁性扁平粉末を熱処理する。熱処理装置について特に制限は無いが、熱処理温度は200℃〜500℃の条件で熱処理されることが好ましい。該当温度で熱処理を行うことによって、保磁力が低下し、高透磁率の軟磁性扁平粉末となる。また、熱処理時間について特に制限は無く、処理量や生産性に応じて適宜選択されるとよい。長時間の熱処理の場合、生産性が低下するため、5時間以内が好適である。 Next, the soft magnetic flat powder is heat-treated. The heat treatment apparatus is not particularly limited, but the heat treatment temperature is preferably 200° C. to 500° C. By performing the heat treatment at the corresponding temperature, the coercive force decreases, and the soft magnetic flat powder with high magnetic permeability is obtained. The heat treatment time is not particularly limited and may be appropriately selected depending on the treatment amount and productivity. In the case of heat treatment for a long time, productivity is reduced, so that it is preferable to be within 5 hours.
本発明に用いられる軟磁性扁平粉末においては、酸化を抑えるために、真空中あるいは不活性ガス中で熱処理されることが好ましい。表面処理の観点から、窒素中ガス中で熱処理されてもよいが、その場合は保磁力の値が上昇し、透磁率は真空で熱処理された場合に比べて低下する傾向にある。
<作用>
The soft magnetic flat powder used in the present invention is preferably heat-treated in vacuum or in an inert gas in order to suppress oxidation. From the viewpoint of surface treatment, the heat treatment may be performed in a gas in nitrogen, but in that case, the value of the coercive force increases, and the magnetic permeability tends to be lower than that in the case of heat treatment in vacuum.
<Action>
軟磁性扁平粉末の平均粒径D50は35〜55μmであることが好ましく、40〜50μmであることがより好ましい。平均粒径が35μm未満では、アスペクト比の高い扁平粉が得られ難く、実部透磁率μ′が低くなる傾向がある。平均粒径が大きくなりすぎると、シート成型が困難になるため好ましくない。特に、平均粒径が55μmを超えると、シート表面の凹凸が目立つ傾向があり、これを防ぐために特別な処理が必要となり、性能面、コスト面で好ましくない。 The average particle diameter D 50 of the soft magnetic flat powder is preferably 35 to 55 μm, more preferably 40 to 50 μm. If the average particle size is less than 35 μm, it is difficult to obtain a flat powder having a high aspect ratio, and the real part permeability μ′ tends to be low. If the average particle size becomes too large, it becomes difficult to form the sheet, which is not preferable. In particular, if the average particle size exceeds 55 μm, irregularities on the sheet surface tend to be conspicuous, and special treatment is required to prevent this, which is not preferable in terms of performance and cost.
軟磁性扁平粉末のタップ密度TDは0.6〜1.0g/ccであることが好ましく、0.7〜0.9g/ccであることがより好ましい。タップ密度は加工が進むほど単調低下する傾向にあり、0.6g/cc未満では、長時間の加工になり、平均粒径の低下と保磁力の上昇をもたらすため好ましくない。また、タップ密度が1.0g/ccを超えると、平均粒径が大きくなる傾向があり、シートへの充填率が低くなり性能面で好ましくない。 The tap density TD of the soft magnetic flat powder is preferably 0.6 to 1.0 g/cc, and more preferably 0.7 to 0.9 g/cc. The tap density tends to decrease monotonically as the processing progresses, and if it is less than 0.6 g/cc, it takes a long time to process, which is not preferable because the average particle diameter decreases and the coercive force increases. If the tap density exceeds 1.0 g/cc, the average particle size tends to increase, and the filling rate into the sheet decreases, which is not preferable in terms of performance.
軟磁性扁平粉末の保磁力Hcは、239〜479A/mであることが好ましく、319〜439A/mであることがより好ましい。保磁力Hcが239A/m未満では、低周波数帯で複素透磁率(μ=μ′―jμ″)の虚数部μ″の値が大きくなるため、エネルギーロスが大きくなる。また、保磁力Hcが479A/mを超えると、複素透磁率(μ=μ′―jμ″)の実数部μ′の値が小さくなるため、アンテナ性能が悪くなる。 The coercive force Hc of the soft magnetic flat powder is preferably 239 to 479 A/m, more preferably 319 to 439 A/m. When the coercive force Hc is less than 239 A/m, the value of the imaginary part μ″ of the complex magnetic permeability (μ=μ′−jμ″) increases in the low frequency band, resulting in a large energy loss. Further, when the coercive force Hc exceeds 479 A/m, the value of the real part μ′ of the complex magnetic permeability (μ=μ′−jμ″) becomes small, and the antenna performance deteriorates.
軟磁性扁平粉末の厚さ方向に磁場を印加して測定した保磁力が、長手方向に磁場を印加して測定した保磁力の2〜4.5倍であることが好ましく、2〜3.5倍であることがより好ましく、2〜3倍であることがさらに好ましい。2未満では透磁率が低くなり、4.5を超えるとシートの表面に突起が多く発生するため成形性が悪化する可能性がある。 The coercive force measured by applying a magnetic field in the thickness direction of the soft magnetic flat powder is preferably 2 to 4.5 times the coercive force measured by applying a magnetic field in the longitudinal direction, and 2 to 3.5. It is more preferable that it is double, and it is further preferable that it is 2-3 times. If it is less than 2, the magnetic permeability is low, and if it exceeds 4.5, many protrusions are generated on the surface of the sheet, which may deteriorate the formability.
軟磁性扁平粉末のXRDに起因するピークの最強ピーク(2θ=44±2°)に関して,半価幅が0.3〜0.6であることが好ましく、0.4〜0.5であることがより好ましい。半価幅が0.3未満では、扁平粉末に過剰な熱処理を施すことになるため、保磁力Hcが極端に小さくなる。そのため、複素透磁率(μ=μ′―jμ″)の虚数部μ″の値が大きくなり、エネルギーロスが大きくなる。また、半価幅が0.6を超えると、アトライタ加工により発生した扁平粉末中の格子欠陥の回復が不十分になるため、μ′が低くなり、アンテナとしての性能を発揮できない。 Regarding the strongest peak (2θ=44±2°) of the peak due to XRD of the soft magnetic flat powder, the half width is preferably 0.3 to 0.6, and 0.4 to 0.5. Is more preferable. If the full width at half maximum is less than 0.3, the flat powder is subjected to excessive heat treatment, and the coercive force Hc becomes extremely small. Therefore, the value of the imaginary part μ″ of the complex magnetic permeability (μ=μ′−jμ″) becomes large and the energy loss becomes large. On the other hand, if the full width at half maximum exceeds 0.6, recovery of lattice defects in the flat powder generated by the attritor processing becomes insufficient, and μ'becomes low, so that the performance as an antenna cannot be exhibited.
水アトマイズ法またはガスアトマイズ法またはディスクアトマイズ法と溶融による合金化後の粉砕法により、本発明の扁平粉末を作製しやすい。また、アトマイズにより製造された粉末は形状が球状に近いことからアトライタ加工による粉砕よりも扁平化が進行しやすい。粉砕法により製造された粉末は粒径がアトマイズ粉末よりも小さいことから、シート表面の突起発生が抑制される傾向がある。 The flat powder of the present invention can be easily produced by a water atomizing method, a gas atomizing method, a disk atomizing method, and a pulverizing method after alloying by melting. In addition, since the powder produced by atomization has a shape close to a sphere, flattening is more likely to occur than crushing by attritor processing. Since the powder produced by the pulverization method has a smaller particle size than the atomized powder, the generation of protrusions on the sheet surface tends to be suppressed.
本発明を真空またはアルゴン、窒素雰囲気のいずれかで熱処理することで、アトライタ加工で発生した扁平粉末中の格子欠陥を回復し、透磁率を回復する。熱処理雰囲気が大気の場合、酸化が進み、本発明の粉末が作製できない。したがって、真空または不活性雰囲気での熱処理が必要になる。また、窒素雰囲気での熱処理で窒化被膜を形成させ、表面抵抗の高い粉末の作製が可能である。これにより、うず電流の発生が抑えられ、RFID等の10MHz帯前後で使用されるアンテナとしての性能が向上する傾向がある。 By subjecting the present invention to heat treatment in a vacuum or in an atmosphere of argon or nitrogen, the lattice defects in the flat powder generated by the attritor processing are recovered and the magnetic permeability is recovered. When the heat treatment atmosphere is the air, oxidation progresses and the powder of the present invention cannot be produced. Therefore, heat treatment in a vacuum or an inert atmosphere is required. Further, it is possible to produce a powder having high surface resistance by forming a nitride film by heat treatment in a nitrogen atmosphere. As a result, the generation of eddy current is suppressed, and the performance as an antenna used in the 10 MHz band around RFID or the like tends to be improved.
軟磁性扁平粉末の熱処理温度は200〜500℃であることが好ましく、350〜450℃であることがより好ましい。本発明において、熱処理はアトライタ加工で発生した扁平粉末中の格子欠陥を回復し、保磁力を低下させるための工程であるため、200℃では不十分である。また、500℃を超えると、材料の組成によっては焼結を起こすことがあり、それが粗大な塊となってシートの表面に突起が多く発生する。 The heat treatment temperature of the soft magnetic flat powder is preferably 200 to 500°C, more preferably 350 to 450°C. In the present invention, the heat treatment is a step for recovering the lattice defects in the flat powder generated by the attritor processing and lowering the coercive force, and therefore 200° C. is insufficient. On the other hand, when the temperature exceeds 500° C., sintering may occur depending on the composition of the material, which becomes coarse lumps and many protrusions are generated on the surface of the sheet.
本発明の軟磁性扁平粉末においては、平均粒子径D50とタップ密度TDの比(D50/TD)、及び、扁平粉末の長手方向に磁場を印加して測定した保磁力が請求項1で表される条件を満足するものである。また、シート成型後の絶縁性を高めるなどの観点においては、表面処理された粉末が好適となる場合があり、本発明の扁平加工方法で製造された粉末について、熱処理工程中あるいは熱処理工程の前後において、表面処理工程を必要に応じて加えても良い。たとえば表面処理のために、活性ガスを微量に含む雰囲気下で熱処理されてもよい。 In the soft magnetic flat powder of the present invention, the ratio of the average particle diameter D50 to the tap density TD (D50/TD) and the coercive force measured by applying a magnetic field in the longitudinal direction of the flat powder are represented by claim 1. It satisfies the condition that Further, from the viewpoint of enhancing the insulating property after sheet molding, the surface-treated powder may be suitable, and for the powder produced by the flattening method of the present invention, during the heat treatment step or before and after the heat treatment step. In, a surface treatment step may be added if necessary. For example, for surface treatment, heat treatment may be performed in an atmosphere containing a small amount of active gas.
また、従来から提案されているシアン系カップリング剤に代表される表面処理により、耐食性やゴムへの分散性を改善することも可能である。また、磁性シートの製造方法も従来提案されている方法で可能である。例えば、トルエンに塩素化ポリエチレンなどを溶解したものに扁平粉末を混合し、これを塗布、乾燥させたものを各種のプレスやロールで圧縮することで製造可能である。 Further, it is possible to improve the corrosion resistance and the dispersibility in rubber by the surface treatment represented by the conventionally proposed cyan coupling agent. Further, the method of manufacturing the magnetic sheet may be a conventionally proposed method. For example, it can be produced by mixing a flat powder in a mixture of chlorinated polyethylene and the like in toluene, applying and drying the flat powder, and compressing it with various presses and rolls.
以下、本発明について、実施例によって具体的に説明する。
(扁平粉末の作製)
水アトマイズ法またはガスアトマイズ法またはディスクアトマイズ法と溶融による合金化後の粉砕法のいずれかにより所定の成分の粉末を作製し150μm以下に分級した。ガスアトマイズは、アルミナ製坩堝を溶解に用い、坩堝下の直径5mmのノズルから合金溶湯を出湯し、これに高圧アルゴンを噴霧することで実施した。これを原料粉末としアトライタにより扁平加工した。アトライタは、SUJ2製の直径4.8mmのボールを使用し、原料粉末と工業エタノールとともに攪拌容器に投入し、羽根の回転数を300rpmとして実施した。
Hereinafter, the present invention will be specifically described with reference to Examples.
(Preparation of flat powder)
Powders of predetermined components were prepared by any of the water atomizing method, gas atomizing method, disk atomizing method, and pulverizing method after alloying by melting, and classified to 150 μm or less. Gas atomization was carried out by using an alumina crucible for melting, discharging a molten alloy from a nozzle having a diameter of 5 mm under the crucible, and spraying high-pressure argon onto the molten alloy. This was used as a raw material powder and flattened by an attritor. As the attritor, balls made of SUJ2 and having a diameter of 4.8 mm were used, the raw material powder and industrial ethanol were put into a stirring container, and the rotation speed of the blade was set to 300 rpm.
工業エタノールの添加量は、原料粉末100質量部に対し、200〜500質量部とした。扁平化助剤は、添加しないか、もしくは原料粉末100質量部に対し、1〜5質量部とした。扁平加工後に攪拌容器から取り出した扁平粉末と工業エタノールをステンレス製の皿に移し、80℃で24時間乾燥させた。このようにして得た扁平粉末を真空中またはアルゴン中または窒素中で、200〜500℃で2時間熱処理し、各種の評価に用いた。 The amount of industrial ethanol added was 200 to 500 parts by mass with respect to 100 parts by mass of the raw material powder. The flattening aid was not added, or was 1 to 5 parts by mass with respect to 100 parts by mass of the raw material powder. The flat powder and industrial ethanol taken out from the stirring container after flattening were transferred to a stainless steel dish and dried at 80° C. for 24 hours. The flat powder thus obtained was heat-treated at 200 to 500° C. for 2 hours in vacuum, argon or nitrogen, and used for various evaluations.
ディスクアトマイズは、アルミナ製坩堝を溶解に用い、坩堝下の直径1〜5mmのノズ
ルから合金溶湯を出湯し、高速で回転するディスクの上に落とすことで実施した。回転速度は、40000rpmから60000rpmである。ディスクによって合金溶湯は急冷され、凝固して、粉末が得られる。アトライタによる扁平加工と熱処理は、ガスアトマイズの時と同様の条件であり、各種の評価に用いた。
The disk atomization was performed by using an alumina crucible for melting, discharging the molten alloy from a nozzle having a diameter of 1 to 5 mm below the crucible, and dropping the molten alloy onto a disk rotating at high speed. The rotation speed is 40,000 rpm to 60,000 rpm. The alloy melt is rapidly cooled by the disk and solidifies to obtain a powder. The flattening by the attritor and the heat treatment were under the same conditions as in gas atomization, and were used for various evaluations.
(扁平粉末の評価)
得られた扁平粉末の平均粒径、タップ密度、保磁力、透磁率を評価した。平均粒径はレーザー回折法、真密度はガス置換法で評価した。タップ密度は、約20gの扁平粉末を、容積100cm3のシリンダーに充填し、落下高さ10mmタップ回数200回の時の充填密度で評価した。保磁力は直径6mm、高さ8mmの樹脂製容器に扁平粉末を充填し、この容器の高さ方向に磁化した場合と直径方向に磁化した場合の値を測定した。なお、扁平粉末は充填された円柱の高さ方向が厚さ方向となっているため、容器の高さ方向に磁化した場合が扁平粉末の厚さ方向、容器の直径方向に磁化した場合が扁平粉末の長手方向の保磁力となる。印加磁場は144kA/mで実施した。
(Evaluation of flat powder)
The average particle size, tap density, coercive force, and magnetic permeability of the obtained flat powder were evaluated. The average particle size was evaluated by a laser diffraction method, and the true density was evaluated by a gas replacement method. The tap density was evaluated by filling about 20 g of flat powder into a cylinder having a volume of 100 cm 3 and filling density when the drop height was 10 mm and the number of taps was 200 times. The coercive force was measured by filling a resin container having a diameter of 6 mm and a height of 8 mm with flat powder, and magnetizing the container in the height direction and in the diameter direction. In addition, since the height direction of the filled cylinder of the flat powder is the thickness direction, the flat powder is magnetized in the height direction of the container and the flat powder is magnetized in the diameter direction of the container. It becomes the coercive force in the longitudinal direction of the powder. The applied magnetic field was 144 kA/m.
(磁性シートの作製および評価)
トルエンに塩素化ポリエチレンを溶解し、これに得られた扁平粉末を混合、分散した。この分散液をポリエステル樹脂に厚さ100μm程度に塗布し、常温常湿で乾燥させた。その後、130℃、15MPaの圧力でプレス加工し、磁性シートを得た。磁性シートのサイズは150mm×150mmで厚さは50μmである。なお、磁性シート中の扁平粉末の体積充填率はいずれも約50%であった。次に、この磁性シートを、外径7mm、内径3mmのドーナツ状に切り出し、インピーダンス測定器により、室温で13.56MHzにおけるインピーダンス特性を測定し、その結果から透磁率(複素透磁率の実数部:μ′,複素透磁率の虚数部:μ″)を算出した。
(Preparation and evaluation of magnetic sheet)
Chlorinated polyethylene was dissolved in toluene, and the resulting flat powder was mixed and dispersed. This dispersion was applied to a polyester resin to a thickness of about 100 μm and dried at room temperature and normal humidity. Then, it pressed at 130 degreeC and the pressure of 15 MPa, and obtained the magnetic sheet. The size of the magnetic sheet is 150 mm×150 mm and the thickness is 50 μm. The volume filling rate of the flat powder in each magnetic sheet was about 50%. Next, this magnetic sheet was cut into a donut shape having an outer diameter of 7 mm and an inner diameter of 3 mm, and the impedance characteristic at 13.56 MHz was measured at room temperature with an impedance measuring device. From the result, the magnetic permeability (the real part of the complex magnetic permeability: μ′, the imaginary part of the complex permeability: μ″) was calculated.
以上、本発明を実施例に基づいて説明したが、本発明はこの実施例に特に限定されない。また、比較例は、後述の表1、2に示す条件を適宜異ならせて作製した。表1、2に評価結果を示す。 The present invention has been described above based on the embodiment, but the present invention is not particularly limited to this embodiment. Further, the comparative example was produced by appropriately changing the conditions shown in Tables 1 and 2 described later. Tables 1 and 2 show the evaluation results.
表1、2に示す比較例No.1〜2は、平均粒径D50の値が小さいために、扁平粉末のアスペクト比が小さくなるため、磁性シート形成時の透磁率が小さくなる。また、平均粒径D50とタップ密度TDの比が小さく、かつ厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.3は、平均粒径D50とタップ密度TDの比が小さく、かつ厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。 Comparative example Nos. shown in Tables 1 and 2. In Nos. 1 and 2, the average particle diameter D 50 was small, and the aspect ratio of the flat powder was small, so that the magnetic permeability during the formation of the magnetic sheet was small. Further, since the ratio of the average particle diameter D 50 to the tap density TD is small and the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2, the magnetic permeability is low. Comparative Example No. No. 3, the ratio of the average particle diameter D 50 to the tap density TD is small, and the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2, so the magnetic permeability is low.
比較例No.7は、平均粒径D50とタップ密度TDの比が小さく、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。さらに、XRDの最強ピーク(2θ=44±2°の半価幅)幅が0.3未満であるために、扁平粉末に過剰な熱処理を施すことになるため、保磁力のHcが極端に小さくなる。そのために、複素透磁率の虚数部μ〃の値が大きくなり、エネルギーロスが大きくなる。 Comparative Example No. In No. 7, since the ratio of the average particle diameter D 50 to the tap density TD is small and the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex permeability becomes large in the low frequency band, resulting in a large energy loss. Further, the magnetic permeability is low because the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2. Further, the strongest peak of XRD (half-width of 2θ=44±2°) width is 0.3. Since the flat powder is excessively heat-treated, the coercive force Hc becomes extremely small, which increases the value of the imaginary part μ〃 of the complex magnetic permeability, resulting in a large energy loss. Become.
比較例No.8は、No.7と同様に、平均粒径D50とタップ密度TDの比が小さく、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.9は、平均粒径D50とタップ密度TDの比が小さく、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。比較例No.10は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。 Comparative Example No. No. 8 is No. As in No. 7, since the ratio of the average particle diameter D 50 to the tap density TD is small and the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex magnetic permeability in the low frequency band is large, resulting in a large energy loss. Further, the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2. Therefore, the magnetic permeability is low, Comparative Example No. 9 has a small ratio of the average particle diameter D 50 and the tap density TD, Since the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex permeability becomes large in the low frequency band, and the energy loss becomes large. Comparative Example No. In No. 10, since the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex permeability becomes large in the low frequency band, and the energy loss becomes large.
比較例No.13〜14は、平均粒径D50とタップ密度TDの比が小さく、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.15は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.16は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。 Comparative Example No. In Nos. 13 to 14, the ratio of the average particle diameter D 50 to the tap density TD is small, and the coercive force in the longitudinal direction is small. Therefore, the value of the imaginary part μ″ of the complex magnetic permeability is large in the low frequency band, and the energy loss is large. Further, the magnetic permeability is low because the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2. Comparative Example No. 15 has a small coercive force in the longitudinal direction and thus has a complex frequency band in the low frequency band. Since the value of the imaginary part μ″ of the magnetic permeability becomes large, the energy loss becomes large. Further, since the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2, the magnetic permeability is low. Comparative Example No. In No. 16, since the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex permeability becomes large in the low frequency band, and the energy loss becomes large.
比較例No.18は、平均粒径D50とタップ密度TDの比が大きく、かつ平均粒径D50が大きいために、磁性シートの成形性が悪化する可能性がある。比較例No.19は、平均粒径D50が小さいために、扁平粉末のアスペクト比が小さくなるため、磁性シート形成時の透磁率が小さくなる。また、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。さらに、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。さらにまた、XRDの最強ピーク(2θ=44±2°の半価幅)幅が0.6を超えるために、アトライタ加工により発生した偏平粉末中の格子欠陥の回復が不十分になるため、虚数部μ″の値が低くなり、アンテナとしての性能を発揮できない。 Comparative Example No. In No. 18, the ratio of the average particle diameter D 50 to the tap density TD is large, and the average particle diameter D 50 is large, so the moldability of the magnetic sheet may deteriorate. Comparative Example No. In No. 19, since the average particle size D 50 is small, the aspect ratio of the flat powder becomes small, so that the magnetic permeability at the time of forming the magnetic sheet becomes small. In addition, since the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex magnetic permeability is large in the low frequency band, resulting in a large energy loss. Further, the coercive force in the longitudinal direction with respect to the coercive force in the thickness direction is increased. The magnetic permeability is low because the ratio is less than 2. Furthermore, since the XRD strongest peak (half-value width of 2θ=44±2°) width exceeds 0.6, the flat powder in the flat powder generated by the attritor processing Since the recovery of lattice defects becomes insufficient, the value of the imaginary part μ″ becomes low, and the performance as an antenna cannot be exhibited.
比較例No.23は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。比較例No.24は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、XRDの最強ピーク(2θ=44±2°の半価幅)幅が0.3未満であるために、扁平粉末に過剰な熱処理を施すことになるため、保磁力のHcが極端に小さくなる。そのために、複素透磁率の虚数部μ〃の値が大きくなり、エネルギーロスが大きくなる。 Comparative Example No. In No. 23, the coercive force in the longitudinal direction is small, so that the value of the imaginary part μ″ of the complex magnetic permeability is large in the low frequency band, and thus the energy loss is large. In Comparative Example No. 24, the coercive force in the longitudinal direction is small. Therefore, the value of the imaginary part μ″ of the complex permeability becomes large in the low frequency band, resulting in a large energy loss. In addition, since the strongest peak of XRD (half-width of 2θ=44±2°) width is less than 0.3, the flat powder is subjected to excessive heat treatment, so that the coercive force Hc is extremely small. Become. Therefore, the value of the imaginary part μ〃 of the complex magnetic permeability becomes large, and the energy loss becomes large.
比較例No.25は、No.24と同様に、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、XRDの最強ピーク(2θ=44±2°の半価幅)幅が0.3未満であるために、扁平粉末に過剰な熱処理を施すことになるため、保磁力のHcが極端に小さくなる。そのために、複素透磁率の虚数部μ〃の値が大きくなり、エネルギーロスが大きくなる。 Comparative Example No. No. 25 is No. As in No. 24, the coercive force in the longitudinal direction is small, so that the value of the imaginary part μ″ of the complex magnetic permeability is large in the low frequency band, resulting in a large energy loss. Further, the strongest peak of XRD (2θ=44±2) Since the flat powder is excessively heat-treated, the coercive force Hc becomes extremely small, and therefore the imaginary part μ of the complex magnetic permeability μ The value of 〃 increases and the energy loss increases.
比較例No.26は、長手方向の保磁力が小さいために低周波数帯で複素透磁率の虚数部μ″の値が大きくなるためエネルギーロスが大きくなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.31、32、35は、平均粒径D50とタップ密度TDの比が小さく、かつ長手方向の保磁力Hcが479A/mを超えるため複素透磁率の実数部μ′の値が小さくなるため、アンテナ性能が悪くなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。 Comparative Example No. In No. 26, since the coercive force in the longitudinal direction is small, the value of the imaginary part μ″ of the complex magnetic permeability becomes large in the low frequency band, resulting in a large energy loss. In addition, the coercive force in the longitudinal direction relative to the coercive force in the thickness direction. The magnetic permeability is low because the ratio is less than 2. In Comparative Examples Nos. 31, 32, and 35, the ratio of the average particle diameter D 50 to the tap density TD is small, and the coercive force Hc in the longitudinal direction is 479 A/m. Since the value exceeds the real part μ′ of the complex magnetic permeability, the antenna performance deteriorates, and the magnetic permeability decreases because the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2.
比較例No.33、34、36は、長手方向の保磁力Hcが479A/mを超えるため複素透磁率の実数部μ′の値が小さくなるため、アンテナ性能が悪くなる。また、厚さ方向の保磁力に対する長手方向の保磁力の比が2未満のため透磁率が低くなる。比較例No.37〜42は、Fe−Si−Cr系合金での比較である。比較例No.43〜44は、Si含有量が小さい場合であって、その場合のAl含有量が小さい場合と大きい場合であって、これらいずれも結果的に磁性シートの透磁率が小さくなる。また、比較例No.45〜46は、逆に、Si含有量が大きい場合であって、その場合のAl含有量が小さい場合と大きい場合であって、これも同様に、結果的に磁性シートの透磁率が小さくなる。
これに対して、本発明である、No.4〜6、No.11〜12、17、No.20〜22、No.27〜30は、いずれも本発明の条件を満足することから、いずれの効果をも達成することが出来ることが分かる。
Comparative Example No. Since the coercive force Hc in the longitudinal direction of each of 33, 34, and 36 exceeds 479 A/m, the value of the real part μ′ of the complex magnetic permeability becomes small, and the antenna performance deteriorates. Further, since the ratio of the coercive force in the longitudinal direction to the coercive force in the thickness direction is less than 2, the magnetic permeability is low. Comparative Example No. 37 to 42 are comparisons of Fe-Si-Cr alloys. Comparative Example No. In Nos. 43 to 44, the Si content was small, and the Al content in that case was small and the Si content was large, respectively, and as a result, the magnetic permeability of the magnetic sheet becomes small. In addition, Comparative Example No. On the contrary, 45 to 46 are cases where the Si content is large and the Al content in that case is small and the case where the Al content is large, which also results in a small magnetic permeability of the magnetic sheet. ..
On the other hand, according to the present invention, No. 4-6, No. 11-12, 17, No. 20-22, No. Since all of Nos. 27 to 30 satisfy the conditions of the present invention, it can be seen that any effects can be achieved.
以上のように、平均粒径D50とタップ密度TDの比(D50/TD)が35〜92であり、長手方向に磁場を印加して測定した保磁力が239〜479A/mである場合、RFID等の10MHz帯前後での透磁率は、実数部μ′が高く、虚数部μ″が小さい値が得られる。また、厚さ方向の保磁力が長手方向の保磁力の2〜4.5倍の場合、十分に高い複素透磁率を示し、さらに、シート表面の突起を抑制できる。さらに、XRDの最強ピーク(2θ=44±2°)の半価幅が0.3〜0.6の場合、高い複素透磁率を示す等の極めて優れた効果を奏するものである。
特許出願人 山陽特殊製鋼株式会社
代理人 弁理士 椎 名 彊
As described above, the ratio (D 50 /TD) of the average particle diameter D 50 to the tap density TD is 35 to 92, and the coercive force measured by applying a magnetic field in the longitudinal direction is 239 to 479 A/m. , RFID has a high permeability in the vicinity of 10 MHz band, a high real part μ′ and a small imaginary part μ″. Further, the coercive force in the thickness direction is 2 to 4. In the case of 5 times, the complex magnetic permeability is sufficiently high, and the protrusion on the sheet surface can be suppressed, and the full width at half maximum of the strongest peak of XRD (2θ=44±2°) is 0.3 to 0.6. In the case of, it has an extremely excellent effect such as showing a high complex magnetic permeability.
Patent applicant Sanyo Special Steel Co., Ltd.
Attorney Attorney Shiina Akira
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